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dc.contributor.advisorPurcell, W.
dc.contributor.advisorNete, M.
dc.contributor.authorVilakazi, Amanda Qinisile
dc.date.accessioned2019-09-03T09:07:16Z
dc.date.available2019-09-03T09:07:16Z
dc.date.issued2017-07
dc.identifier.urihttp://hdl.handle.net/11660/10326
dc.description.abstractEnglish: The aim of this project was to investigate the dissolution and possible separation of Ti and Fe in ilmenite using eco-friendly and economically viable procedures. Method validation was established with commercial salts such as FeCl3·6H2O and TiCl3 including Ti and Fe metal powders with high purity. The successful procedures were evaluated for the dissolution of ilmenite and subsequent separations of Ti and Fe in the mineral matrix. Dissolution techniques such as open-beaker acid digestion and flux fusion were evaluated. The separation techniques which were investigated include selective precipitation, solvent extraction and ion exchange. Analytical determinations were performed with inductively coupled plasma-optical emission spectroscopy (ICP- OES) while infrared spectroscopic (IR) analyses was used to characterize the Ti and Fe containing compounds. Acid dissolution was investigated with different mineral acids which included aqua regia, HCl, HNO3, H2SO4 and H3PO4. Analytical results showed good average recoveries ranging from 98(1) to 105.2(2) % Ti in TiCl3 and 100(4) to 103(2) % Fe in FeCl3·6H2O after these salts were dissolved in water. The dissolution of the Ti and Fe metal powders was investigated with aqua regia, HCl, HNO3, H2SO4 and H3PO4 and only H2SO4 and H3PO4 successfully dissolves the metal powders and excellent Ti and Fe recoveries of 103.6(5) and 105.2(6) % Ti with 103(2) and 103(2) % Fe were obtained. The dissolution of ilmenite with acid digestion yielded 38.39 % TiO2 and 45.25 % Fe2O3 with H2SO4 and 34.79 % TiO2 and 19.50 % Fe2O3 in H3PO4 with clearly pointed to incomplete sample dissolution. Flux fusion using NH4·HF2, KF, K2S2O7, Na2CO3, LiBO2, Na2B4O7 and phosphate mixture (Na2HPO4/NaH2PO4·H2O) as fluxes was also investigated. Only the borates (LiBO2 and Na2B4O7) and the phosphate flux mixture (Na2HPO4/NaH2PO4·H2O) indicated complete ilmenite dissolution. The quantitative results obtained after the flux fusion method (borates and phosphate), were compared with the non-destructive SEM-EDS semi-quantitative results. Comparative results were obtained for Ti, Mg, Mn and Al with some difference observed in the Fe quantities that were recovered. The separation of Ti and Fe in the ilmenite was further investigated using only the phosphate flux method. Selective precipitation using NaTPB/phenantroline was unsuccessful with both Ti and Fe precipitated in solution. However the use of only NaPT resulted in the complete precipitation of Fe (99.60(1) %) while Ti remained in solution (103(1) %). Separation using solvent extraction indicated that Fe was preferentially isolated with 100 % Fe and 0.00 % Ti and thus achieving a complete separation using NaPT in different organic solvents. Separation of Fe and Ti using the MIBK/NaPT and 1-octanol/NaPT combinations indicated a selective extraction of Fe into the MIBK and 1- octanol with 95.9(3) to 103(3) % Fe and 0.0 to 24(9) % Ti obtained in the organic phase using HCl, H2SO4 and H3PO4, depending on the acid concentrations. Separation factors were calculated to in the range of 1.7 to 8.6 x 107. Solvent extraction using kerosene/TOPO and MIBK/acacH systems indicated a selective extraction of Fe into the organic phase (0.8(1) to 22(6) % Ti and 2(2) to 99.0(8) % Fe in kerosene, 0.7(2) to 7(2) % Ti and 22.5(2) to 100(2) % Fe in MIBK) with separation factors of 1.4 x 102 to 3.3 x 105 in kerosene and 23 x 100 to 1.6 x 105 in MIBK in HCl matrix. The separation of Ti and Fe with strong and weak basic ion exchange resins (Amberlite IRA-900, Amberlite IRA 402, Dowex 1x4 ion exchange resin, weak basic Dowex Marathon WBA and Dowex 66 free base) indicated the successful separations with Ti the strongly retained species during elution with H3PO4 solution. Fe recoveries of 96(1) to 103.46(1) % were obtained for the weak anionic resins using 3.0 and 5.0 M H3PO4 as eluent. The strongly retained Ti was eluted with 5.0 M HCl with recoveries of 99.1(1) to 103(4) %. Recoveries were generally poor with the use of strong anionic exchange resins for both Fe and Ti resins (62(2) to 74(5) % for Fe and 68(4) to 84(3) % for Ti). The separation factor (α) for strong and weak anionic resins were in the range of 1.4 (Fe/Ti) to 6.7 (Fe/Ti) in 3.0 to 10.0 M H3PO4.en_ZA
dc.description.abstractAfrikaans: Die doel van hierdie projek was die ondersoek van die oplos en moontlike skeiding van Ti en Fe in ilmeniet deur van omgewingsvriendelike en ekonomiese prosedures gebruik te maak. Metodevalidasie is met behulp van kommersiële anorganiese soute soos FeCl3·6H2O en TiCl3, asook die suiwer metaalpoeiers van Ti en Fe uitgevoer. Die suksesvolle prosedure is daarna vir die suksesvolle oplos van ilmeniet geëvalueer gevolg deur die skeiding van Ti en Fe in die mineraalmatriks. Oplossingstegnieke soos oop-beker suurvertering en soutsmelting is as oplostegnieke geëvalueer. Die skeidingstegnieke wat ondersoek is, sluit onderandere selektiewe presipitering, vloeistofekstraksie en ioon-uitruiling in. Die kwantifisering van die onderskeie elemente is met behulp van induktief-gekoppelde plasma optiese-emissiespektroskopie (IGP- OES) uitgevoer terwyl infrarooispektroskopie (IR) vir die karakterisering van die onderskeie Ti- en Fe-bevattende verbindings aangewend is. Verskillende mineraalsure koningswater, HCl, HNO3, H2SO4 en H3PO4 insluit, is vir die oop-beker suurvertering van die monsters ondersoek. Analitiese resultate toon dat kwantitatiewe herwinning van die elemente verkry is en herwinnings van 98(1) tot 105.2(2) % is vir Ti in TiCl3 verkry, terwyl tussen 100(4) en 103(2) % Fe in FeCl3·6H2O waargeneem is. Die oplos van die Ti- en Fe-metaalpoeiers is ook met behulp van koningswater, HCl, HNO3, H2SO4 en H3PO4 ondersoek en slegs H2SO4 en H3PO4 was suksesvol in die oplos van die metaalpoeiers. Uitstekende Ti- en Fe-herwinning is met 103.6(5) en 105.2(6) % Ti en 103(2) en 103(2) % Fe in die onderskeie metaalpoeiers verkry. Die oplos van ilmeniet deur suurvertering was onvolledig en het metaalherwinnings van 38.39 % TiO2 en 45.25 % Fe2O3 met H2SO4 gelewer, terwyl H3PO4 slegs 34.79 % TiO2 en 19.50 % Fe2O3 opgelos het. Soutsmelting is met behulp van NH4·HF2, KF, K2S2O7, Na2CO3, LiBO2, Na2B4O7, en fosfaatmengsel (Na2HPO4/NaH2PO4·H2O) ondersoek. Slegs die boraatsoute (LiBO2 en Na2B4O7), asook die alkalimetaal-fosfaatsoute (Na2HPO4/NaH2PO4·H2O) was in staat om die ilmeniet volledig op te los. Die verskillende kwantitatiewe resultate wat met die onderskeie soutsmeltingsprosedures verkry is, is verder met nie-destruktiewe skandeer- elektronmikroskopie asook energieverspreidende spektroskopie (SEM-EVS) vergelyk. Die resultate wat op hierdie twee metodes verkry is (oplos vs nie-oplos) toon vergelelykbare Ti, Mg, Mn en Al hoeveelhede terwyl die Fe waardes tussen die metodes effens verskil het. Die skeiding van Ti en Fe in die ilmeniet is verder slegs met behulp van die fosfaatvloedmetode, ondersoek. Selektiewe presipitering is aanvanklik met met behulp van NaTPB/fenantrolien ondersoek, maar hierdie metode was onsuksesvol aangesien betekenisvolle hoeveelhede Ti en Fe in die presispitaat teenwoordig was. Die gebruik van slegs NaPT as cheleermiddel was uiters susksevol en die Fe (99.60(1) %) het volledig gepresipiteer terwyl die Ti (103(1) %) in die ilmeniet in oplossing gebly het. Skeidingsresultate wat met behulp van vloeistofekstraksie verkry is, dui daarop dat die Fe by voorkeur geïsoleer word met 100 % Fe en 0.00 % Ti en dus is die volledige skeiding van die twee elemente met NaPT opgelos in verskillende organiese oplosmiddels, bewerkstellig. Skeiding van die Fe en Ti deur middel van die MIBK/NaPT en 1-oktanol/NaPT kombinasies dui ook die op selektiewe ekstraksie van Fe in die MIBK en 1-oktanol met 95.9(3) tot 103(3) % Fe terwyl 0.0 tot 24(9) % Ti verkry in die organiese fase in die teenwoordigheid van HCl, H2SO4 en H3PO4, teenwoordig was. Die suurkonsentrasie-variasie het duidelik ʼn invloed op die % metaal in die organiesse fase uitgeoefen en skeidingsfaktore het tussen 1.7 en tot 8.6 x 107 gevarieër. Oplossingsekstraksie met keroseen/TOPO- en MIBK/asasH-stelsels was ook slektied in die ten opsigte van element-ekstraksie en die Ti in die organiese fase het tussen 0.8(1) en 22(6) % gewissel terwyl 2(2) tot 99.0(8) % Fe in keroseen teenwoordig was. In die MIBK sistee het die Ti tussen 0.7(2) tot 7(2) % Ti gewissel terwyl die Fe tussen 22.5(2) tot 100(2) % Fe in gewissel het. Skeidingsfaktore van 1.4 x 102 tot 3.3 x 105 in keroseen en 23 x 100 tot 1.6 x 105 in MIBK in ʼn HCl matriks is bereken. Die skeiding van Ti en Fe met sterk en swak alkaliese ioonuitruilingsharse (Amberlite IRA-900, Amberlite IRA 402, Dowex 1x4 ioonuitruilingshars, swak basiese Dowex Marathon WBA, en Dowex 66 vry-basis) was ook suksesvol in die skeiding van die twee elemente. Resultate het getoon dat Ti die sterkste op die ioonuitruilers geadsorbeer het tydens die eluering met H3PO4. Fe herwinnings wat tussen 96(1) en 103.46(1) % gewissel het, is vir swak alkaliese anioniese harse verkry indien hulle met 3.0 en 5.0 M H3PO4 ge-elueer is. Die sterk ge-adsorbeerde Ti is daarna met 5.0 M HCl geëlueer en herwinnings van 99.1(1) tot 103(4) % is verkry. Die sterk anioniese uitruilingsharse het oor die algemeen swak resultate gelewer en slegs 62(2) tot 74(5) % Fe en 68(4) tot 84(3) % Ti is herwin. Die skeidingsfaktor (α) vir sterk en swak anioniese harse is as 1.4 (Fe /Ti) en 6.7 (Fe / Ti) in 3.0 tot 10.0 M H3PO4 bereken.en_ZA
dc.language.isoenen_ZA
dc.publisherUniversity of the Free Stateen_ZA
dc.subjectDissertation (M.Sc. (Chemistry))--University of the Free State, 2017en_ZA
dc.subjectHydrometallurgyen_ZA
dc.subjectIlmeniteen_ZA
dc.titleHydrometallurgical beneficiation of ilmeniteen_ZA
dc.typeDissertationen_ZA
dc.rights.holderUniversity of the Free Stateen_ZA


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